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Sup Info E Microgels OM Supporting Information to Microgel Size Modulation by Electrochemical Switching Olga Mergel, a Patrick Wünnemann, a Ulrich Simon, b Alexander Böker, c Felix A. Plamper a* a Institute of Physical Chemistry II, RWTH Aachen University, Landoltweg 2, 52056 Aachen, Germany b Institute of Inorganic Chemistry, RWTH Aachen University, Landoltweg 1, 52056 Aachen, Germany c Fraunhofer-Institut für Angewandte Polymerforschung (IAP), Lehrstuhl für Polymermaterialien und Polymertechnologie, Universität Potsdam, Geiselbergstraße 69, 14476 Potsdam, Germany *Corresponding Author: Felix A. Plamper ([email protected]; +49 241 8094750) 1. Materials and Methods Materials. The microgel particles were synthesized by precipitation copolymerization of N-isopropylacrylamide (NiPAM) and N-[3-(dimethylamino)propyl]methacrylamide (DMAPMA) and subsequent quaternization of the DMAPMA comonomer amine function with methyl iodide. A detailed microgel synthesis and characterization is 1 described elsewhere. Potassium chloride (KCl) and potassium hexacyanoferrate(III) (K 3[Fe(CN) 6]) were obtained . from Merck. Potassium hexacyanoferrate(II) trihydrate (K 4[Fe(CN) 6] 3H2O) was purchased from AnalaR NORMAPUR. All chemicals were used as received without any further purification. Deionized water (18.2 MΩ) from Millipore Milli-Q-purification system was distilled twice and used in all experiments. General Electrochemical Techniques. All electrochemical measurements were conducted on the CH Instruments Electrochemical Workstation Potentiostat CHI760D (Austin, Texas, USA). The experiments were performed in a conventional three-electrode setup in a water jacketed cell connected to a thermostat (thermo scientific Haake A28) at 20 °C or at 36 -37 °C in case of electrolysis experiments and at room temperature (23 °C) in case of hydrodynamic voltammetry experiments (for concentration determination of supernatant) and electrochemical impedance spectroscopy. For such hydrodynamic voltammetry experiments, the potentiostat was connected with a rotating ring disk rotator (RRDE-3A from ALS Japan). Two kinds of working electrodes have been used. For hydrodynamic voltammetry experiments, a platinum (rotating) disk electrode, 4 mm disk diameter, was conducted as working electrode. For bulk electrolysis experiments, a platinum gauze electrode (35 mm x 20 mm) was used as working electrode. Furthermore, a spirally platinum electrode, 23 cm (legth), was used for hydrodynamic voltammetry experiments and a platinum wire (50 mm) for electrolysis as counter electrode, which was immersed in 0.025 M, or 0.05 M KCl solution separated by a diaphragm from the remaining compartment (2 half-cell setup). For electrochemical impedance spectroscopy experiments, the platinum gauze electrode served as counter electrode, while the rotating disk electrode (without rotation) was connected as working electrode. An Ag/AgCl electrode stored in 1 M KCl served as reference electrode in all three cases. All potentials in the text and figures are referenced to the Ag/AgCl couple. Electrolysis experiments of an initial solution of 1 mM K 4[Fe(CN) 6] in a supporting electrolyte solution of 0.025 M KCl were performed in presence of the microgel P(NIPAM-co - MAPTAC) (6.3 g / L; 0.63 wt%) with an initial charge ratio of icr = 1, or the double concentrated solution of 2 mM K4[Fe(CN) 6] in 0.05 M KCl in presence of P(NIPAM-co-MAPTAC) microgel (12.5 g / L; 1.25 wt%, icr = 1). The solutions were purged with Ar for 10 min to remove dissolved oxygen. Bulk electrolysis experiments were performed at 20 °C or ~ 37 °C by application of an oxidation potential of 0.6 V to an initial solution containing 0.63 wt% of P(NIPAM-co -MAPTAC) microgel and 1 mM K 4[Fe(CN) 6] in 0.025 M KCl with an initial charge ratio ( icr ) of 1. For stepwise oxidation a charge of -12 to -20 mC for diluted microgel dispersion and -125 to -177 mC for concentrated dispersions was transferred and the microgel size was determined by 3D DLS experiments. This stepwise oxidation was repeated 9 - 10 times. For reduction, a potential of 0 V was applied to the K 3[Fe(CN) 6] containing microgel dispersion. Furthermore, full oxidation and reduction were performed by transfer of ±0.9 C in diluted dispersions (1 mM K 4[Fe(CN) 6]) and ±1.8 C in the concentrated case (2 mM K 4[Fe(CN) 6]). 1 Rotating Disk Electrode (RDE). In order to obtain information about the nominal charge ratio ( ncr ) and thus the amount of the effectively incorporated multivalent counterions, centrifugation experiments (40.000 rpm; 30 °C) of an initial solution of 1 mM K 4[Fe(CN) 6] in 0.025 M KCl in presence of 6.3 g/L P(NIPAM-co -MAPTAC) microgel were performed after oxidation and reduction. Hydrodynamic voltammograms of the supernatant were recorded by sweeping the potential in the range of (-0.1) V - 0.5 V vs. Ag/AgCl at a scan rate of 5 mV s -1. The rotation rate was remained constant at 100 rpm at a temperature of 23 °C. Further, hydrodynamic voltammetry experiments were performed at different electrolysis states: at an intermediate state of 1 mM K 4[Fe(CN) 6], 1 mM K 3[Fe(CN) 6] and at 3- 4- the extreme states of 2 mM [Fe(CN) 6] or 2 mM [Fe(CN) 6] at 37 °C in 0.05 M KCl (100 rpm in presence and absence of microgel; 12.5 g/L P(NIPAM-co -MAPTAC)). Before performing each hydrodynamic voltammetry measurement, the working electrode was polished first with 1 µm diamond and subsequently with 0.05 µm alumina polish, rinsed with water and dried with a stream of argon. Electrochemical Impedance Spectroscopy (EIS) experiments were performed at different electrolysis states. An initial solution of 2 mM K4[Fe(CN) 6] in 0.05 M KCl in presence and absence of the microgel (12.5 g/L P(NIPAM-co - MAPTAC) was oxidized at 37 °C, while impedance spectroscopy experiments were performed in steps of -300 mC 4- transferred charge. In order to measure the extreme stages of switching, 2 mM [Fe(CN) 6] in 0.05 M KCl, or 2 mM 3- [Fe(CN) 6] in 0.05 M KCl (in presence and absence of microgel) were prepared freshly and were not electrolyzed before the impedance spectroscopy experiment. The (dc) potential was held at the open circuit potential measured at each electrolysis stage, while a small oscillating voltage of 5 mV amplitude was applied (leading to an alternating current – ac – readout). The measuring frequency f used for EIS measurements ranged from 1 Hz to 100 kHz. As fit model, the modified Randles circuit was used, in accordance to our previous publication. 1 Impedance data analysis was performed according to proper transfer function derivation and identification procedures, which involved complex nonlinear last-squares (CNLS) fitting based on the Marquardt-Levenberg algorithm using the CH Instruments Beta software. Electrophoretic mobility . Measurements of the electrophoretic mobility were performed on a NanoZS Zetasizer (Malvern). Zeta-Potential was derived by use of the Smoluchowski limit. Measurements were performed in disposable capillary cells (Malvern, DTS1061C). Electrophoretic mobility was measured at an angle of 17° at a wavelength of the laser beam was 633 nm. Measurements were performed at 25 °C. 3D cross correlation dynamic light scattering (3D-DLS) setup was used for the determination of the hydrodynamic radii, as the samples were turbid. All experiments were performed on an LS instruments setup (Fribourg, Switzerland) equipped with a 633 nm HeNe laser (JDS Uniphase, KOHERAS GmbH, 25 mV, Type LGTC 685-35), a goniometer (ALV, CGS-8F), digital Hardware correlator (ALV 7004, ALV GmbH, Langen, Germany), two avalanche photo diodes (Perkin Elmer, Type SPCM-AQR-13-FC), light scattering electronics (ALV, LSE-5004), an external programmable thermostat (Julabo F32) and an index-match-bath filled with toluene. Angle- and temperature-dependent measurements were recorded in pseudo-cross correlation mode varying the scattering angle from 45 to 105 ° at 5 ° intervals including a variation of temperature (in the range of 20 to 60 °C at 2 K intervals for temperature-dependent experiments and measurement time of 200 s). For experiments at a constant temperature of ~ 37 °C, the scattering angle was varied from 45 to 102 ° at 3 ° intervals. For data evaluation, the decay rate (first cumulant) from second order cumulant fit was plotted against the squared length of the scattering vector q2. The data were fitted with a homogeneous linear regression, whereas the diffusion coefficient was extracted from the slope and the hydrodynamic radius Rh calculated by using the Stokes-Einstein equation. Scanning Force Microscopy (SFM). The swelling behavior of the microgels was observed with a liquid-cell AFM (Veeco Dimension Icon) to mimic bulk solution conditions. A temperature-controlled stage (ICONEC-V2-NOPOT, Bruker AXS) was used to equilibrate the custom-made cell before each measurement for ~ 90 min. The microgels were analyzed with MSCT-A (Bruker AXS) tips (spring constant 0.07 N/m, resonant frequency 22 kHz) at 25 °C and 37 °C via Peak Force QNM. For the liquid-cell experiments, 20 µl of an aqueous dispersion were spincoated at 2000 rpm for 45 s onto a silicon wafer, which was cleaned with toluene (ISO, VWR), dried with a CO 2 jet system and activated via plasma treatment for 30 s (Plasma Activate Flecto 10 USB, 100 W, 0.2 mbar) before deposition. This silicon wafer was immersed in a two-chamber homemade measurement cell. The chambers were separated by a dialysis membrane in order to equilibrate both chambers. One part was filled with double concentration of microgels, whereas the wafer was placed into the other part for SFM investigations. The concentrations of salts (and the average microgel concentration) were basically the same as for the bulk electrolysis experiments. After data extraction from the AFM images via Nanoscope 8.15 (Bruker AXS), the average microgel height profile was 2 calculated from a number of single microgels (typically 6 microgels).
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